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POTASSIUM HYDROXIDE PELLETS SEMI C39-0699 © SEMI 1 978, 1999 1 SEMI C39-0699 SPECIFICA TION FOR POTASSIUM HYDROXIDE PELLETS This spe cifica tion was te chnically approve d by the G lobal Process Che micals Com mittee and…

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SEMI C38-0699 © SEMI 1991, 19993
NOTICE: These standards do not purport to address
safety issues, if any, associated with their use. It is the
responsibility of the user of these standards to establish
appropriate safety and health practices and determine
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suitability of the standards set forth herein for any
particular application. The determination of the
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mentioned herein. These standards are subject to
change without notice.
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compliance with this standard may require use of
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Copyright by SEMI® (Semiconductor Equipment and Materials
International), 3081 Zanker Road, San Jose, CA 95134. Reproduction o
f
the contents in whole or in part is forbidden without express written
consent of SEMI.
POTASSIUM HYDROXIDE PELLETS SEMI C39-0699 © SEMI 1978, 19991
SEMI C39-0699
SPECIFICATION FOR POTASSIUM HYDROXIDE PELLETS
This specification was technically approved by the Global Process Chemicals Committee and is the direct
responsibility of the North American Process Chemicals Committee. Current edition approved by the North
American Regional Standards Committee on April 23, 1999. Initially available on SEMI OnLine May 1999;
to be published June 1999. This document replaces SEMI C1.14 in its entirety. Originally published in
1978.
1 Purpose
1.1 The purpose of this document is to standardize
requirements for potassium hydroxide pellets used in
the semiconductor industry and testing procedures to
support those standards. Test methods have been shown
to give statistically valid results. This document also
provides guidelines for grades of potassium hydroxide
pellets for which a need has been identified. In the case
of the guidelines, the test methods may not have been
statistically validated yet.
2 Scope
2.1 The scope of this document is all grades of
potassium hydroxide pellets used in the semiconductor
industry.
3 Limitations
3.1 None.
4 Referenced Documents
SEMI C1 — Specifications for Reagents
5 Terminology
5.1 None.
6 Physical Property (for information only)
6.1 Not applicable.
7 Requirements
7.1 The requirements for potassium hydroxide pellets
for Grade 1 are listed in Table 1.
8 Grade 1 Procedures
8.1 Assay — Weigh accurately 35 to 40 g of sample in
a closed weighing bottle. Transfer to a 500 mL
volumetric flask, dissolve in carbon dioxide-free water,
cool to 25°C, dilute to the mark with carbon dioxide
free water, and mix thoroughly. Transfer 25.0 mL of
this solution to a 500 mL glass-stoppered flask, dilute
with 175 mL of carbon dioxide-free water, add 5 mL of
barium chloride reagent solution, shake, and allow to
stand for five minutes. Add 0.15 mL of phenolphthalein
indicator solution and titrate with 1 N hydrochloric
acid. (Save this solution for the potassium carbonate
test.)
% Assay
=
mL
×
N
o
f
H
Cl
×
112
.
2
Weight of sample g
()
8.2 Potassium Carbonate (K
2
CO
3
) — To the above ti-
trated solution, add 0.15 mL of methyl orange indicator
solution and continue the titration with 1 N hydro-
chloric acid. The additional hydrochloric acid is equiv-
alent to that consumed by the potassium carbonate.
% K
2
CO
3
=
mL
×
N
×
H
Cl
×
138
.
2
Weight of sample g
()
8.3 Ammonium Hydroxide Precipitate — Weigh about
10 g of sample and dissolve in about 100 mL of water.
8.3.1 Cautiously add 12 mL of sulfuric acid to 15 mL
of water, cool, then cautiously add the mixture to the
solution of the sample and evaporate to dense fumes.
Cool, dissolve the residue in 130 mL of hot water, and
add ammonium hydroxide until the solution is just basic
to methyl red.
8.3.2 Heat to boiling, filter, wash with hot water, and
ignite. The weight of the residue should not exceed 2
mg.
8.4 Insoluble Matter — Dissolve 50 g of sample in
250 mL of carbon dioxide-free water in a 500 mL
stoppered flask and cool to 25°C. The solution should
be clear and colorless. Filter through a tared, medium-
porosity filtering crucible and wash thoroughly with hot
water. Dry the crucible at 105°C for 1 hour, cool, and
weigh the residue. The weight of the residue should not
exceed 2.5 mg.
8.5 Stock Solution for 8.6-8.11, 8.13-8.14 — Dissolve
50 g of sample in 250 mL of carbon dioxide-free water
and dilute with such water to 500 mL. One mL contains
0.10 g of sample. Store in a plastic container.
8.6 Nitrogen Compounds — Dilute 20 mL of the
Stock Solution with 50 mL of water in a flask
connected through a spray trap to a condenser, the end
of which dips beneath the surface of 10 mL of 0.1 N
hydrochloric acid. For the standard, take 50 mL of
water in a similar flask, and add 10 mL of the Stock
Solution and 1 mL of the nitrogen standard solution. To
each flask add 0.5 g of aluminum wire in small pieces,
SEMI C39-0699 © SEMI 1978, 1999 POTASSIUM HYDROXIDE PELLETS2
allow to stand for 1 hour, and slowly distill about 35
mL. To each distillate add 2 mL of freshly boiled 10%
sodium hydroxide reagent solution, dilute with water to
50 mL, and add 2 mL of Nessler reagent. Any color in
the solution of the sample should not exceed that in the
standard.
8.7 Chloride — Dilute 10 mL of the Stock Solution
with water to 50 mL. Filter if necessary through a
chloride-free filter. To 10 mL of this solution, add 5 mL
of water, 2 mL of nitric acid, and 1 mL of silver nitrate
reagent solution. Any turbidity developed should not
exceed that produced by 0.02 mg of chloride ion (Cl) in
an equal volume of solution containing the quantities of
reagent used in the test.
8.8 Phosphate — To 40 mL of the Stock Solution, add
10 mL of hydrochloric acid and evaporate to dryness on
a steam bath. Dissolve the residue in 25 mL of 0.5 N
sulfuric acid. Add 1 mL of ammonium molybdate
reagent solution and 1 mL of p-(methylamino)phenol
sulfate reagent solution. Allow to stand for 2 hours at
room temperature. Any blue color developed should not
exceed that produced when 0.02 mg of phosphate ion
(PO
4
) is treated as the sample.
8.9 Sulfate — To 20 mL of the Stock Solution, add 5
mL of hydrochloric acid and evaporate to dryness on a
steam bath. Dissolve the residue in 20 mL of water and
evaporate again to dryness. Dissolve the residue in 20
mL of water, filter if necessary, and add 1 mL of dilute
hydrochloric acid (1 + 19) and 1 mL of barium chloride
reagent solution. Allow to stand for 10 minutes. Any
turbidity developed should not exceed that produced
when 0.04 mg of sulfate ion (SO
4
) is treated as the
sample.
8.10 Heavy Metals (as Ag) — To 60 mL of the Stock
Solution cautiously add 15 mL of nitric acid. For the
standard add 0.05 mg of silver ion (Ag) to 10 mL of the
Stock Solution and cautiously add 15 mL of nitric acid.
Evaporate both solutions to dryness over a low flame or
on an electric hot plate. Dissolve each residue in about
20 mL of water, filter if necessary through a chloride-
free filter, and dilute with water to 25 mL. Adjust the
pH of the standard and sample solutions to between 3
and 4 (using a pH meter) with 1 N acetic acid or
ammonium hydroxide (10% NH
3
). Dilute each solution
with water to 40 mL and stir. Add 10 mL of freshly
prepared hydrogen sulfide water to each solution and
stir again. Any color developed in the sample should
not exceed that in the standard.
8.11 Iron — Neutralize 10 mL of the Stock Solution
with hydrochloric acid, using phenolphthalein indicator
solution, add 2 mL in excess, and dilute with water to
50 mL. Add 30 to 50 mg of ammonium peroxydisulfate
crystals and 3 mL of ammonium thiocyanate reagent
solution. Any red color developed should not exceed
that produced when 0.01 mg of iron ion (Fe) is treated
as the sample.
8.12 Mercury — To each of two thoroughly clean 125
mL conical flasks add 20 mL of water and 1 mL of 4%
potassium permanganate solution. To one add 5.5 g of
solid sample. To the other add 0.5 g of sample and 0.5
mg of mercury ion (Hg). To each flask slowly add 18
mL of hydrochloric acid, with constant swirling. Heat
to boiling, allow to cool, and dilute to 100 mL.
Determine mercury in 10 mL aliquots by the cold vapor
(flameless) atomic absorption method using 1 mL of
10% hydroxylamine hydrochloride reagent solution and
2 mL of 10% stannous chloride reagent solution for the
reduction. The peak obtained with the sample solution
should not be larger than that from the standard
mercury solution.
8.13 Nickel — Dilute 20 mL of the Stock Solution to
50 mL with water and neutralize with hydrochloric
acid. Dilute to 85 mL and add ammonium hydroxide to
make the solution barely basic (pH 8). Add 5 mL of
bromine water and 5 mL of alcoholic 1%
dimethylglyoxime solution. Any red color developed
should not exceed that produced when 0.02 mg of
nickel ion (Ni) is treated as the sample.
8.14 Sodium — Dilute 10 mL of the Stock Solution
with water to 100 mL to form the Sample Solution. To
prepare the Standard Solution, add 0.5 mg of sodium
ion (Na) to 10 mL of the Stock Solution and dilute with
water to 100 mL.
8.14.1 Using flame emission spectroscopy, observe
the emission of the Standard Solution at the 589 nm
sodium line. Observe the emission of the Sample
Solution at the 589 nm sodium line and also at a
wavelength of 580 nm. The difference between the
intensities observed for the Sample Solution at 580 nm
and 589 nm should not exceed the difference observed
at 589 nm between the Sample Solution and the
Standard Solution (see SEMI C1, Section 3.7, Flame
Emission Spectroscopy).
9 Grade 2 Procedures
9.1 This section does not apply to this chemical.
10 Grade 3 Procedures
10.1 This section does not apply to this chemical.
11 Grade 4 Procedures
11.1 This section does not apply to this chemical.
12 Grade 5 Procedures
12.1 This section does not apply to this chemical.